WO2012121154A1 - Base, substrat comportant une couche cristalline de nitrure de gallium et procédé pour sa production - Google Patents
Base, substrat comportant une couche cristalline de nitrure de gallium et procédé pour sa production Download PDFInfo
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- WO2012121154A1 WO2012121154A1 PCT/JP2012/055407 JP2012055407W WO2012121154A1 WO 2012121154 A1 WO2012121154 A1 WO 2012121154A1 JP 2012055407 W JP2012055407 W JP 2012055407W WO 2012121154 A1 WO2012121154 A1 WO 2012121154A1
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- 239000013078 crystal Substances 0.000 title claims abstract description 245
- 239000000758 substrate Substances 0.000 title claims abstract description 213
- 229910002601 GaN Inorganic materials 0.000 title claims abstract description 179
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 title claims abstract description 177
- 238000000034 method Methods 0.000 title claims abstract description 17
- 229910052594 sapphire Inorganic materials 0.000 claims abstract description 126
- 239000010980 sapphire Substances 0.000 claims abstract description 126
- 238000004519 manufacturing process Methods 0.000 claims description 14
- 229910052733 gallium Inorganic materials 0.000 claims description 2
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims 1
- 238000005121 nitriding Methods 0.000 claims 1
- 239000012159 carrier gas Substances 0.000 description 13
- 238000005530 etching Methods 0.000 description 10
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- 230000010287 polarization Effects 0.000 description 9
- 239000004065 semiconductor Substances 0.000 description 9
- XCZXGTMEAKBVPV-UHFFFAOYSA-N trimethylgallium Chemical group C[Ga](C)C XCZXGTMEAKBVPV-UHFFFAOYSA-N 0.000 description 7
- 230000000873 masking effect Effects 0.000 description 6
- 238000001020 plasma etching Methods 0.000 description 5
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 238000000927 vapour-phase epitaxy Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
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- 229910021478 group 5 element Inorganic materials 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000002248 hydride vapour-phase epitaxy Methods 0.000 description 3
- 230000002401 inhibitory effect Effects 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
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- 238000002488 metal-organic chemical vapour deposition Methods 0.000 description 3
- 238000001451 molecular beam epitaxy Methods 0.000 description 3
- 229920002120 photoresistant polymer Polymers 0.000 description 3
- 230000005701 quantum confined stark effect Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 230000001133 acceleration Effects 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000004020 luminiscence type Methods 0.000 description 2
- 125000004433 nitrogen atom Chemical group N* 0.000 description 2
- 230000002269 spontaneous effect Effects 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
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- 239000011248 coating agent Substances 0.000 description 1
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000001039 wet etching Methods 0.000 description 1
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- H01L29/02—Semiconductor bodies ; Multistep manufacturing processes therefor
- H01L29/12—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed
- H01L29/20—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by the materials of which they are formed including, apart from doping materials or other impurities, only AIIIBV compounds
- H01L29/2003—Nitride compounds
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- C—CHEMISTRY; METALLURGY
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- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
- C30B25/18—Epitaxial-layer growth characterised by the substrate
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/34—Nitrides
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- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/38—Nitrides
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
- C30B29/403—AIII-nitrides
- C30B29/406—Gallium nitride
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- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02612—Formation types
- H01L21/02617—Deposition types
- H01L21/02636—Selective deposition, e.g. simultaneous growth of mono- and non-monocrystalline semiconductor materials
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- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02612—Formation types
- H01L21/02617—Deposition types
- H01L21/02636—Selective deposition, e.g. simultaneous growth of mono- and non-monocrystalline semiconductor materials
- H01L21/02647—Lateral overgrowth
- H01L21/0265—Pendeoepitaxy
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- H—ELECTRICITY
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- H01S—DEVICES USING THE PROCESS OF LIGHT AMPLIFICATION BY STIMULATED EMISSION OF RADIATION [LASER] TO AMPLIFY OR GENERATE LIGHT; DEVICES USING STIMULATED EMISSION OF ELECTROMAGNETIC RADIATION IN WAVE RANGES OTHER THAN OPTICAL
- H01S2304/00—Special growth methods for semiconductor lasers
- H01S2304/12—Pendeo epitaxial lateral overgrowth [ELOG], e.g. for growing GaN based blue laser diodes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
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- Y10T428/24479—Structurally defined web or sheet [e.g., overall dimension, etc.] including variation in thickness
- Y10T428/2457—Parallel ribs and/or grooves
Definitions
- the present invention relates to a base substrate, a gallium nitride crystal multilayer substrate, and more particularly to a multilayer substrate in which a gallium nitride (GaN) crystal layer having a low threading dislocation density is stacked on a sapphire base substrate, and a method for manufacturing the same.
- GaN gallium nitride
- any GaN layer has crystal growth of GaN in the axial direction, and the surface is a c-plane ( ⁇ OOO1> plane).
- the piezoelectric polarization generated by the compressive strain applied to the InGaN quantum well layer is superimposed on the InGaN quantum well layer, Therefore, a large internal polarization electric field is generated in the c-axis direction. Under the influence of this internal polarization electric field, the quantum confined Stark Effect (QCSE) is considered to cause problems such as peak emission wavelength shift due to decrease in luminous efficiency and increase in required injection current. It has been.
- QCSE quantum confined Stark Effect
- an InGaN layer is formed on the a-plane: ⁇ 11-20> plane or m-plane: ⁇ 1-100> plane, which is a nonpolar plane of the GaN crystal, and spontaneously It has been studied to avoid the influence of an internal electric field in which polarization and piezoelectric polarization are superimposed (see Patent Documents 1 to 3).
- an InGaN quantum well layer is formed on a plane called a semipolar plane inclined about 60 degrees in the a-axis or m-axis direction, for example, a semipolar ⁇ 11-22> plane, thereby It has also been studied to avoid the influence of internal electrodes (Non-patent document 1, Non-patent document 2).
- the substrate is said to have a threading dislocation density of about 2 to 3 ⁇ 10 8 pieces / cm 2, and a crystal substrate having a high crystal quality with a lower threading dislocation density is desired.
- Non-polar surface of GaN crystal such as a substrate having a low threading dislocation density and a high crystal quality such as a-plane or m-plane, or a substrate having ⁇ 11-22> or ⁇ 10-11> plane
- Another object of the present invention is to provide a GaN crystal multilayer substrate in which a GaN crystal layer having a semipolar plane as a main surface is laminated on a sapphire base substrate, a manufacturing method thereof, and a sapphire base substrate used in the manufacturing method.
- the present inventors have studied a method of growing a GaN crystal having a desired crystal plane using a sapphire base substrate having a plurality of concave grooves as a starting point from the side wall surface of the groove of the base substrate.
- the size of the crystal growth region on the side wall of the groove greatly affects the crystal quality (threading dislocation density), while it has little effect on the surface flatness of the grown crystal and the crystallinity evaluated by X-ray diffraction measurement.
- the present invention has been completed.
- the present invention includes a sapphire base substrate and a gallium nitride crystal layer formed by crystal growth on the base substrate, and a plurality of the gallium nitride crystal layers are formed on the main surface of the sapphire base substrate.
- the crystal is grown laterally starting from the side wall of the groove and the surface is formed in parallel to the main surface, and the dark spot density of the gallium nitride crystal is less than 2 ⁇ 10 8 pieces / cm 2 .
- the dark spot density of the gallium nitride crystal is 1.4 ⁇ 10 8 pieces / cm 2 or less
- the gallium nitride crystal layer is a gallium nitride crystal layer comprising a surface having a nonpolar or semipolar plane orientation
- a plurality of grooves having sidewalls inclined with respect to the main surface of the underlying substrate are formed on a sapphire base substrate, and a gallium nitride crystal is selectively grown laterally starting from the sidewalls of the groove.
- a method for producing a gallium nitride crystal multilayer substrate characterized in that the width (d) of the region on the side wall on which the gallium nitride crystal is grown is set to 10 to 750 nm.
- the width (d) of the region in which the gallium nitride crystal is grown is 100 to 200 nm, 5) It is preferable that the side wall from which the lateral crystal growth from the groove portion starts is the c-plane of the sapphire single crystal.
- the dark spot density of the gallium nitride crystal is less than 2 ⁇ 10 8 pieces / cm 2 , preferably 1.85 ⁇ 10 8 pieces / cm 2 or less, particularly preferably 1.4 ⁇ 10 8. Since it is 8 pieces / cm 2 or less and the crystal quality is high, the light emitting efficiency of a semiconductor light emitting device such as an LED or LD manufactured using the laminated substrate is improved. Further, by selectively growing a gallium nitride crystal from the side wall of the groove formed on the sapphire base substrate, a high-quality gallium nitride crystal having a nonpolar or semipolar surface as a main surface can be obtained. For this reason, the semiconductor light-emitting device manufactured using this is less affected by the decrease in light emission efficiency due to the quantum confined Stark effect than the conventional gallium nitride crystal layer substrate having the c-plane as the main surface.
- the gallium nitride crystal multilayer substrate of the present invention has a plurality of groove portions having side walls inclined with respect to the main surface of the base substrate, and a width (d) of 10 to 750 nm for growing a gallium nitride crystal on the side walls of the groove portions.
- a sapphire base substrate provided with a growth region is used as a lower layer, and the surface thereof is formed in parallel with the main surface by lateral crystal growth (ELO) starting from the side wall. It has a structure in which gallium nitride crystal layers having a dark spot density of less than 2 ⁇ 10 8 pieces / cm 2 are stacked.
- the dark spot density is a physical property value that serves as an index for indicating the density of threading dislocations, which are dislocation defects in the crystal, and is measured using a scanning electron microscope / cathode luminescence (SEM / CL) apparatus.
- SEM / CL scanning electron microscope / cathode luminescence
- As a measurement sample a sample in which an n-type GaN crystal layer is stacked on an undoped GaN crystal layer is used, and measurement is performed on the surface of the n-type GaN layer.
- the acceleration voltage during measurement is 5 kV, and the observation range is 20 ⁇ m ⁇ 20 ⁇ m. At this time, the dark spot density is calculated from the total number of dark spots observed within the observation range.
- the sapphire base substrate for producing the crystal laminated substrate of the present invention has a plurality of groove portions having side walls inclined with respect to the main surface of the substrate on the sapphire substrate, and selectively gallium nitride crystals on the side walls of the groove portions.
- the width (d) of the region in which is grown is set to 10 to 750 nm.
- a sapphire substrate whose main surface has a specific plane orientation is used. However, in order to obtain a desired GaN crystal to be described later, it may be a miscut surface inclined at a predetermined angle with respect to the crystal axis.
- a disk-shaped substrate having a thickness of 0.3 to 3.0 mm and a diameter of 50 to 300 mm is usually used.
- an arbitrary plane orientation is selected according to the crystal plane of the target GaN crystal.
- the main surface of the sapphire base substrate is set to ⁇ 10-12>.
- the main surface of the sapphire base substrate is set to ⁇ 11-23>.
- the ⁇ 10-10> plane, the ⁇ 11-20> plane, the ⁇ 20-21> plane, and the like can be main surfaces.
- sapphire c-plane a sapphire substrate having a ⁇ 10-12> plane as a main surface and a c-plane of sapphire single crystal (hereinafter referred to as sapphire c-plane) is formed on a part of the side wall of the groove.
- the angle formed by the main surface of the sapphire substrate is 57.6 degrees.
- the angle formed between the ⁇ 11-22> plane of the target GaN crystal and the c plane of the GaN crystal is 58.4 degrees
- a ⁇ 11-22> plane GaN crystal layer grows with an inclination of 0.8 degrees with respect to the sapphire main surface.
- a miscut substrate having an off angle with the ⁇ 10-12> plane is used, and the ⁇ 11-22> plane, which is the surface of the GaN crystal layer, is parallel to the main surface of the sapphire substrate.
- Various miscut substrates designed so that the surface of the GaN crystal layer is parallel to the main surface of the sapphire base substrate depending on the plane orientation of the target GaN crystal and the surface orientation of the sapphire base substrate used are used. be able to.
- a plurality of grooves are provided in parallel on the main surface of the sapphire base substrate.
- the opening width of the groove is not particularly limited, and is usually set in the range of 0.5 to 10 ⁇ m.
- the interval between the groove portions that is, the interval between the adjacent groove portions and the groove portion on the base substrate main surface line is 1 to 100 ⁇ m.
- the lateral width of the bottom surface of the groove that is, the distance (w) in the direction perpendicular to the extending direction of the groove is not particularly limited, and is generally 1 to 100,000 ⁇ m.
- the number of grooves on the main surface can be arbitrarily set according to the desired area of the GaN crystal to be formed. However, in consideration of the width of the opening, the interval between the grooves, and the width of the bottom surface, it is usually per 1 mm. About 10 to 500 may be provided.
- the groove has a side wall inclined at a predetermined angle with respect to the base substrate main surface, As shown in FIG. 3, the cross-sectional shape is tapered so as to narrow the groove width from the groove opening toward the groove bottom. As shown in FIG. 3, the inclination angle means an angle ( ⁇ ) formed between the main surface of the base substrate and the extended surface of the groove side wall. The angle is determined in consideration of the surface orientation of the GaN crystal to be formed in accordance with the surface orientation of the base substrate main surface.
- this angle is set to 58.4 degrees
- the GaN crystal is grown so that the c-axis of the GaN crystal is in the same direction as the c-axis of the sapphire base substrate to obtain a desired crystal.
- the angle 58.4 degrees at this time is formed by the ⁇ 11-22> plane that is the principal surface of the desired GaN crystal and the c-plane of the GaN crystal that is perpendicular to the c-axis of the GaN crystal that is the growth direction.
- the angle is determined from being 58.4 degrees.
- the angle formed between the ⁇ 10-12> plane, which is the main surface of the sapphire base substrate used, and the sapphire c-plane appearing on the side wall of the groove is 57.6 degrees
- the angle ( ⁇ ) is 57.6 degrees
- the surface of the GaN crystal layer grown thereon is inclined by about 0.8 degrees with respect to the main surface of the sapphire base substrate. Therefore, by using a miscut substrate in which the main surface of the substrate is an off-angle with respect to the sapphire ⁇ 10-12> surface so as to cancel out this angle, the ⁇ 11-22> surface of the GaN crystal becomes the sapphire base.
- a GaN crystal layer grown so as to be parallel to the main surface of the substrate can be obtained.
- this angle is set to 62.0 degrees
- the crystal is grown so that the c-axis of the GaN crystal is in the same direction as the c-axis of the sapphire base substrate to obtain a desired crystal.
- the angle 62.0 degrees at this time is formed by the ⁇ 10-11> plane that is the principal surface of the desired GaN crystal and the c-plane of the GaN crystal that is perpendicular to the c-axis of the GaN crystal that is the growth direction.
- the angle is determined from 62.0 degrees.
- the angle formed between the ⁇ 11-23> plane, which is the main surface of the sapphire base substrate used, and the sapphire c-plane appearing on the side wall of the groove is 61.2 degrees
- the angle ( ⁇ ) is 61.2 degrees
- the surface of the GaN crystal layer grown thereon is inclined about 0.8 degrees with respect to the main surface of the sapphire base substrate. Therefore, by using a miscut substrate in which the main surface of the substrate has an off-angle with respect to the sapphire ⁇ 11-23> surface so as to cancel this angle, the ⁇ 10-11> surface of the GaN crystal becomes the sapphire base.
- a GaN crystal layer grown so as to be parallel to the main surface of the substrate can be obtained.
- the angle of 90 degrees is the angle formed between the ⁇ 11-20> plane that is the principal surface of the desired GaN crystal and the c-plane of the GaN crystal that is perpendicular to the c-axis of the GaN crystal that is the growth direction. , 90 degrees.
- the etching proceeds not only in the direction perpendicular to the main surface of the sapphire substrate but also in a direction other than the vertical including the parallel direction. It is technically difficult to form a groove portion having an angle ( ⁇ ) of 90 degrees, that is, forming a groove portion whose groove side wall is truly perpendicular to the main surface of the sapphire substrate.
- a GaN crystal is formed on the sapphire base substrate having the ⁇ 11-20> plane as the main surface.
- a GaN crystal layer grown so that the ⁇ 10-10> plane is parallel to the main surface of the sapphire base substrate can be obtained.
- the angle of 90 degrees is the angle formed between the ⁇ 10-10> plane that is the principal surface of the desired GaN crystal and the c-plane of the GaN crystal that is perpendicular to the c-axis of the GaN crystal that is the growth direction. , 90 degrees.
- the angle of 90 degrees is the angle formed between the ⁇ 10-10> plane that is the principal surface of the desired GaN crystal and the c-plane of the GaN crystal that is perpendicular to the c-axis of the GaN crystal that is the growth direction. , 90 degrees.
- the setting of the width (d) of the GaN crystal growth region (hereinafter referred to as crystal growth region) on the sidewall of the groove is extremely important for reducing the threading dislocation density.
- the width (d) of the crystal growth region means that when the entire side wall region that is the growth starting point is the crystal growth region, the side where the main substrate main surface and the side wall intersect, the side wall and the groove bottom surface The shortest distance (interval) on the side wall between the intersecting sides.
- the distance (d) obtained by removing the width of the masking portion from the shortest distance (interval) is referred to.
- the width (d) needs to be set to 10 to 750 nm in order to make the dark spot density less than 2 ⁇ 10 8 pieces / cm 2 .
- the width (d) needs to be 100 to 200 nm.
- the lower limit of the width (d) is not particularly limited and is preferably as small as possible. However, the lower limit of the width (d) is determined based on technical restrictions in manufacturing the groove described below.
- the groove portion having the sidewall having the predetermined inclination angle is formed by patterning a photoresist in which only a portion where the groove portion is to be formed becomes an open portion, the photoresist is used as an etching resist, and the sapphire base substrate is subjected to reactive ion etching (Reactive Ion Etching). : RIE) or other dry etching or wet etching.
- control means such as the width of the side wall, the width of the groove opening, the space between the grooves, and the width of the bottom surface, the photoresist coating amount, baking temperature, baking time, UV irradiation amount, UV, Examples include the shape of a photomask when irradiating.
- the etching stage it can be controlled by the etching gas type, etching gas concentration, etching gas mixture ratio, antenna power, bias power, etching time, and the like.
- the width of the side wall which is important in the present invention, can be controlled by obtaining an etching rate, which is the rate at which sapphire is etched per unit time, and changing the etching time.
- a base substrate having side walls of various plane orientations can be created by selecting the main surface of the sapphire base substrate and setting the direction in which the groove extends. Specifically, when the base substrate main surface is the ⁇ 10-12> plane and the extending direction of the groove is the ⁇ 11-20> plane orientation, that is, the a-axis direction, The c-plane is exposed. When the underlying substrate main surface is the ⁇ 11-23> plane and the extending direction of the groove is the ⁇ 10-10> plane orientation, that is, the m-axis direction, the c-plane is exposed on the side wall that is the crystal growth surface. .
- the underlying substrate main surface is the ⁇ 11-20> plane and the extending direction of the groove is the ⁇ 10-10> plane orientation, that is, the m-axis direction
- the c-plane is exposed on the side wall that is the crystal growth surface.
- the base substrate main surface is the ⁇ 10-10> plane and the extending direction of the groove is the ⁇ 11-20> plane orientation, that is, the a-axis direction
- the c-plane is exposed on the side wall which is the crystal growth surface.
- the base substrate main surface is the ⁇ 0002> plane and the extending direction of the groove is the ⁇ 10-10> plane orientation, that is, the m-axis direction
- the a-plane is exposed on the side wall which is the crystal growth plane.
- the sapphire base substrate can be arbitrarily designed with respect to the surface orientation of its main surface and the surface orientation of the side wall that becomes the crystal growth starting surface.
- the sidewalls having various plane orientations lateral growth starting from the c-plane sidewall is likely to occur preferentially and easily controlled. Therefore, it is a preferable aspect to form a side wall composed of the c-plane on at least a part of the side wall constituting the groove.
- SiO 2 film, SiN x , film, TiO 2 film, ZrO 2 is formed in a region other than the crystal growth region by a method such as vacuum deposition, sputtering, or CVD (Chemical Vapor Deposition).
- CVD Chemical Vapor Deposition
- the thickness of the masking layer is usually O.D. It is about 01 to 3 ⁇ m.
- the GaN crystal layer is crystal-grown in the lateral direction by ELO starting from the side wall, and its surface is formed on the sapphire base substrate in parallel with the main surface of the base substrate.
- the thickness of the GaN crystal layer to be formed (height from the main surface of the sapphire base substrate) is not particularly limited, but is usually 2 to 20 ⁇ m.
- the plane orientation of the crystal surface of the GaN crystal layer corresponds to the main surface of the sapphire base substrate, as described above, and includes the ⁇ 11-22> plane, the ⁇ 10-11> plane, the ⁇ 20-21> plane, and the like.
- the growth method of the GaN crystal is not particularly limited, and metal organic vapor phase epitaxy (Metal Organic Vapor Phase Epitaxy: MOVPE), molecular beam epitaxy (Molecular Beam Epitaxy: MBE), hydride vapor phase epitaxy (Hydride Vapor Phase Epitaxy) : HVPE), among which the metalorganic vapor phase epitaxy is the most common.
- MOVPE Metal Organic Vapor Phase Epitaxy
- MBE molecular beam epitaxy
- HVPE hydride vapor phase epitaxy
- the technique described in WO2010 / 023846 proposed by the inventors of the present invention can be applied mutatis mutandis without any limitation.
- the MOVPE apparatus used for crystal growth is mainly composed of a substrate transport system, a substrate heating system, a gas supply system, and a gas exhaust system, all of which are electronically controlled.
- the substrate heating system is composed of a thermocouple, a resistance heater, and a carbon or SiC susceptor provided thereon, and a quartz tray on which the sapphire base substrate of the present invention is set on the susceptor is conveyed. Then, epitaxial growth of the semiconductor layer is performed.
- This substrate heating system is installed in a quartz double tube or a stainless steel reaction vessel equipped with a water cooling mechanism, and a carrier gas and various source gases are supplied into the double tube or reaction vessel.
- a quartz flow channel is used to realize a laminar gas flow on the substrate.
- the carrier gas include H 2 and N 2 .
- An example of the nitrogen element supply source is NH 3 .
- An example of the Ga element supply source is trimethylgallium (TMG).
- the sapphire base substrate is set on a quartz tray so that the main surface of the sapphire faces upward, and then the sapphire base substrate is heated to 1050 to 1150 degrees and the pressure in the reaction vessel is set to 10 to 100 kPa.
- the sapphire base substrate is thermally cleaned by circulating H 2 as a carrier gas in a flow channel installed inside and maintaining that state for several minutes.
- the temperature of the sapphire base substrate is set to 1050 to 1150 degrees
- the pressure in the reaction vessel is set to 10 to 100 kPa
- the carrier gas H 2 is circulated at a flow rate of 10 L / min in the reaction vessel, and NH 3 and TMG are supplied in O.D.
- the flow rate is 1 to 5 L / min and 10 to 150 ⁇ mol / min.
- undoped GaN is heteroepitaxially grown on the side wall of the groove of the sapphire base substrate.
- a GaN layer grows in the normal direction of the main surface of the substrate, and as shown in FIG. 6, a GaN crystal layer is formed on the sapphire base substrate to obtain a laminated substrate.
- the layer thickness of the GaN crystal layer is about 2 to 20 ⁇ m.
- the growth temperature is controlled in order to control the growth from the side wall of the groove without causing growth from the main surface of the substrate. It is necessary to optimize various conditions such as growth pressure, raw material gas supply amount, raw material gas supply ratio, carrier gas type, and carrier gas amount. After determining the growth method, reaction apparatus, raw material, and the like to be used, the conditions may be determined in advance through preliminary experiments.
- the sapphire base substrate used in the present invention may be one in which, for example, the main surface is covered with a crystal growth inhibiting layer made of SiO 2 or the like other than the region for crystal growth. By providing the crystal growth inhibition layer, it is possible to suppress the growth from the main surface of the substrate and control the growth to be preferentially performed from the side wall of the groove.
- the GaN crystal has a base substrate main surface, a groove sidewall exposed from the sapphire c surface, and the other groove sidewall.
- crystal growth from it is necessary to optimize the above various growth conditions in order to control the growth so as to preferentially occur from the groove side wall where the sapphire c-plane is exposed.
- the growth from the main surface of the base substrate can be suppressed by providing a crystal growth inhibiting layer.
- the GaN crystal may grow from the base substrate main surface and the groove side wall.
- the groove side walls on both sides have the same plane orientation, it is necessary to control so that the GaN crystal having the same plane orientation grows from either side and the crystal grows from either side wall of the trench.
- the growth from the main surface of the base substrate may be suppressed. In order to suppress the growth from the main surface of the base substrate, it is effective to provide a crystal growth inhibiting layer, but control is possible only by optimizing the above various growth conditions.
- the GaN crystal layer is constituted by an aggregate of a plurality of band-like GaN crystals grown from the growth region on the side wall of the groove, or by an integrated body in which the band-like GaN crystals are linked together.
- the surface orientation of the surface of the obtained GaN crystal layer varies depending on the crystal structure of the sapphire base substrate. For example, when the main surface of the sapphire base substrate is the ⁇ 10-12> plane and the side wall that serves as the growth origin is the c plane, the a axis of sapphire and the m axis of the GaN crystal are parallel on the side wall surface.
- a GaN crystal having a crystal orientation relationship in which the m-axis of sapphire and the a-axis of the GaN crystal are parallel grows.
- a GaN crystal layer grown so that the ⁇ 11-22> plane of the GaN crystal is parallel to the main surface of the sapphire base substrate is formed on the sapphire base substrate.
- the main surface of the sapphire base substrate is the ⁇ 11-23> plane and the side wall serving as the growth origin is the c-plane
- the m-axis of sapphire and the a-axis of the GaN crystal are parallel on the side wall surface.
- a GaN crystal in which the a-axis of sapphire and the m-axis of the GaN crystal are parallel to each other is crystal-grown.
- the gallium nitride crystal multilayer substrate obtained by the above various growth methods can be used as it is as a substrate for various semiconductor light emitting devices.
- Example 1 [Production of sapphire base substrate] A resist was patterned on the stripe on the ⁇ 10-12> plane sapphire base substrate, and then dry etching was performed by reactive ion etching (RIE) to form a plurality of grooves on the sapphire base substrate.
- the groove portion was formed so that the groove opening width was 3 ⁇ m, the groove depth was 100 nm, and the width of the main surface portion of the substrate to the adjacent groove portion was 3 ⁇ m.
- the inclination angle of the side wall is about 60 degrees, and the width (d) of the side wall calculated from the groove depth and the inclination angle of the side wall is 115 nm. After dry etching, the resist was washed away to obtain a sapphire base substrate.
- This sapphire base substrate has 8466 grooves on the main surface of the substrate.
- the groove is composed of a side wall made of a sapphire c-plane serving as a crystal growth region, a side wall having another plane orientation, and a bottom surface of the groove.
- the prepared sapphire base substrate is set in a MOVPE apparatus on a quartz tray so that the substrate surface faces upward, and then the substrate is heated to 1150 ° C. and the pressure in the reaction vessel is set to 100 kPa.
- the substrate was thermally cleaned by circulating H 2 at 10 L / min as a carrier gas and maintaining this state for 10 minutes.
- the pressure in the reaction vessel was 100kPa while the temperature of the substrate and 460 ° C., while also a flow of carrier gas to circulate inside the reaction vessel at a flow rate of H 2 5L / min, there Group V element source ( NH 3 ) and a group III element supply source (TMG) were deposited at about 25 nm of amorphous GaN on the substrate with respective supply amounts of 5 L / min and 5.5 ⁇ mol / min. Subsequently, the temperature of the substrate is set to 1075 ° C., the pressure in the reaction vessel is set to 20 kPa, and the carrier gas flowing in the reaction vessel is set to H 2 , and the carrier gas is circulated at a flow rate of 5 L / min.
- the GaN deposited on was recrystallized to selectively form GaN crystal nuclei in the crystal growth region on the side wall of the groove.
- the temperature of the base substrate is set to 1075 ° C.
- the pressure in the reaction vessel is set to 20 kPa
- the carrier gas flowing through the reaction vessel is set to H 2 , while flowing at a flow rate of 5 L / min.
- a group V element supply source NH 3
- a group III element supply source TMG
- An undoped GaN crystal was grown to form a GaN crystal layer on the substrate so that lateral crystal growth occurred from the side wall of the groove of the base substrate.
- the temperature of the base substrate is set to 1025 ° C.
- the pressure in the reaction vessel is set to 20 kPa
- the carrier gas flowing through the reaction vessel is set to H 2 , while flowing at a flow rate of 5 L / min.
- a group V element supply source (NH 3 ) and a group III element supply source (TMG) for 300 minutes so that the respective supply amounts are 2 L / min and 30 ⁇ mol / min, and growing a GaN crystal.
- the GaN crystals grown from the side walls of the groove portions of the base substrate were associated with each other to form a GaN crystal layer in which the surface composed of the ⁇ 11-22> plane of the GaN crystal was formed parallel to the main surface of the base substrate.
- n-type GaN crystal layer [Formation of n-type GaN crystal layer]
- the temperature of the substrate is set to 1025 ° C.
- the pressure in the reaction vessel is set to 20 kPa
- the carrier gas to be circulated in the reaction vessel is set to H 2 , while being circulated at a flow rate of 5 L / min.
- Group element supply source (NH 3 ), Group III element supply source (TMG), and n-type doping element supply source (SiH 4 ) are supplied at 2 L / min, 30 ⁇ mol / min, and 5.8 ⁇ 10, respectively.
- An n-type GaN crystal layer epitaxially grown in the same plane orientation as the undoped GaN crystal layer was formed on the undoped GaN crystal layer at a flow rate of ⁇ 3 ⁇ mol / min for 60 minutes.
- Example 2 A GaN crystal layer was formed on the sapphire base substrate in the same manner as in Example 1 except that the groove depth of the groove formed on the sapphire base substrate was 200 nm and the side wall width (d) was adjusted to 231 nm. .
- Example 3 A GaN crystal layer was formed on the sapphire base substrate in the same manner as in Example 1 except that the groove depth of the groove formed on the sapphire base substrate was 500 nm and the side wall width (d) was adjusted to 587 nm. .
- Comparative Example 1 A GaN crystal layer was formed on the sapphire base substrate in the same manner as in Example 1 except that the groove depth of the groove formed on the sapphire base substrate was 1 ⁇ m and the side wall width (d) was adjusted to 1155 nm. .
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Abstract
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KR1020137022202A KR20140019328A (ko) | 2011-03-07 | 2012-03-02 | 하지 기판, 질화갈륨 결정 적층 기판 및 그의 제조 방법 |
CN2012800080170A CN103348044A (zh) | 2011-03-07 | 2012-03-02 | 基底基板、氮化镓晶体层叠基板及其制造方法 |
US13/983,257 US20130313567A1 (en) | 2011-03-07 | 2012-03-02 | Base substrate, gallium nitride crystal multi-layer substrate and production process therefor |
EP12755674.4A EP2684988A1 (fr) | 2011-03-07 | 2012-03-02 | Base, substrat comportant une couche cristalline de nitrure de gallium et procédé pour sa production |
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US20130313567A1 (en) | 2013-11-28 |
KR20140019328A (ko) | 2014-02-14 |
CN103348044A (zh) | 2013-10-09 |
TW201245515A (en) | 2012-11-16 |
EP2684988A1 (fr) | 2014-01-15 |
JP2012184144A (ja) | 2012-09-27 |
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